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Table of contents
Abstract...4
Acknowledgements and dedications...5
Table of contents...6 List of Figures...9 List of Tables...13 List of Equations...15 List of Photographs...16 I. INTRODUCTION...17 1. General introduction...17
II. LITERATURE REVIEW...19
2. Glass-ceramics science...19
2.1 General...19
2.2 Fundamentals of glass-ceramics materials...20
2.2.1 The nature of glass...20
2.2.2 Crystallization of glass...24
A. Nucleation...25
B. Crystal growth...30
2.3 Characterization of lithium silicate and lithium alumina-silicate glass-ceramics...31
2.3.1 Glasses for production glass-ceramics...31
2.3.2 Nucleating agents used in lithium silicate and alumina-silicate systems...34
2.3.3 Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC)...37
2.3.4 Heat treatment inducing nucleation and crystallization process...39
2.3.5 Applications of lithium di-silicate and alumina-silicate glass-ceramics...43
2.4 Transparent glass-ceramics...46
2.5 Dental restoration...49
2.5.1 History of dental restoration...50
2.5.2 Products used for dental restorations...51
2.6 Improvement of mechanical properties upon ion-exchange...53
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2.6.2 The phenomena of decrystallization...57
AIM AND THESIS...59
III. MATERIALS AND METHODS...61
3. Preparation and characterization of materials...61
3.1 Preparation of parent glasses...61
3.1.1 Glass melting...61 3.1.2 Specimen preparation...62 3.2 Glass-ceramics production...63 3.2.1 Thermal analysis...63 3.2.2 Heat treatment...64 3.3 Characterization techniques...65 3.3.1 Mechanical properties...65 3.3.2 X-ray diffraction...66
3.3.3 Nuclear magnetic resonance (NMR)...67
3.3.4 Scanning electron microscopy (SEM)...67
3.3.5 UV/VIS spectrophotometry...68
3.3.6 Dilatometric measurements...68
3.3.7 Chemical solubility...69
3.4 Ion-exchange process...69
3.4.1 Secondary ion mass spectrometry (SIMS)...70
3.4.2 Inductively coupled plasma atomic emission spectroscopy (ICP-AES)...70
3.4.3 Raman spectroscopy...70
IV. RESULTS AND DISCUSSION...71
4. Materials production and examinations...71
4.1 Parent glasses...71
4.1.1 Selection of glass components and representative chemical compositions...71
4.2 Thermal analysis and prior characterization of selected glasses...76
4.2.1 The primary glasses of ratios: Li2O:Al2O3 = 1, Li2O:Al2O3< 1, Li2O:Al2O3> 1 (IIb, IIb/1 and IIb/2)...76
4.2.2 The glasses of the ratio Li2O:Al2O3>1 (IIb/Mod9; IL/IIb)...81
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4.3 Selection of optimum chemical compositions of parent glasses...96
4.4 Thermal analysis of IIb/Mod7 and IIb/Mod10 glasses...97
4.4.1 Identifying suitable nucleation temperature for IIb/Mod7...98
4.4.2 Identifying suitable temperature/time crystallization profile for IIb/Mod7...103
4.4.3 Calculation of Crystallization Activation Energy for IIb/Mod7...104
4.4.4 Thermal analysis - evaluation of thermal treatment of chosen glass IIb/Mod10...109
4.4.5 Identifying suitable nucleation temperature for IIb/Mod10...110
4.4.6 Calculation of Crystallization Activation Energy for IIb/Mod10...111
4.5 Accurate characterization of IIb/Mod7 and IIb/Mod10 parameters...113
4.5.1 Mechanical properties...114
A. IIb/Mod7 glass and glass-ceramics...114
B. IIb/Mod10 glass and glass-ceramics...119
4.5.2 X-ray diffraction...123
4.5.3 Nuclear magnetic resonance (NMR)...133
4.5.4 Scanning electron microscopy (SEM)...135
4.5.5 UV/VIS spectrophotometry...139
4.5.6 Dilatometric analysis...143
4.5.7 Chemical solubility...145
4.6 Characterization of ion-exchanged IIb/Mod7 and IIb/Mod10 glass and glass-ceramics...146
4.6.1 Mechanical properties of glass and glass-ceramics upon ion-exchange...147
4.6.2 Secondary ion mass spectrometry (SIMS)...150
4.6.3 Inductively coupled plasma atomic emission spectroscopy (ICP-AES)...153
4.6.4 X-ray diffraction...153 4.6.5 Raman spectroscopy...155 4.6.6 UV-VIS Spectrophotometry...156 4.6.7 Summation...157 5. Conclusions...158 References...161
